Pyridine → HCID 43654432、化合物
反応式
[Br:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][CH:3]=1.N1C=CC=CC=1.[Cl:15][CH2:16][CH2:17][CH2:18][S:19](Cl)(=[O:21])=[O:20]>C(Cl)Cl.C(OCC)(=O)C>[Br:1][C:2]1[CH:8]=[CH:7][C:5]([NH:6][S:19]([CH2:18][CH2:17][CH2:16][Cl:15])(=[O:21])=[O:20])=[CH:4][CH:3]=1参加物
6
実験手順
4-Bromoaniline (0.86 g, 5.0 mmol) was dissolved in CH2Cl2 (15 mL), pyridine (0.5 mL) was added, and 3-chloropropanesulfonyl chloride (0.6 mL, 5.0 mmol) was added. The mixture was stirred for 4 hours, diluted with ethyl acetate, and then washed with water, 2N HCl, brine, dried over MgSO4, and concentrated. The crude product was purified via Isco chromatography (the Redisep® column, silica, gradient 5-60% ethyl acetate in hexane) to afford 1.2 g (77%) N-(4-bromophenyl)-3-chloropropane-1-sulfonamide.
後処理
- washwashed with water, 2N HCl, brine
- dry with materialdried over MgSO4
- concentrationconcentrated
- customThe crude product was purified via Isco chromatography (the Redisep® column, silica, gradient 5-60% ethyl acetate in hexane)
出典と根拠
- ORDレコード
- ord-4d28705e4e464e3db9f3097137583003
- 出典データセット
- uspto-grants-2007_11
- 特許番号
- US07291643B2
反応ノート
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